Ethylene Oxide → 2-(3,3-Dimethylmorpholin-4-yl)ethan-1-ol
反応式
[CH3:1][C:2]1([CH3:8])[CH2:7][O:6][CH2:5][CH2:4][NH:3]1.[CH3:9][C:10](C)=[O:11].C(=O)=O.C1OC1>CO>[CH3:1][C:2]1([CH3:8])[CH2:7][O:6][CH2:5][CH2:4][N:3]1[CH2:9][CH2:10][OH:11]参加物
5
実験手順
In a pressure vessel containing 3,3-dimethylmorpholine (12.15 g, 106 mmol) in MeOH (17 mL) at −78° C. (external temperature, acetone/CO2(s)) was added ethylene oxide (6.2 mL, 125 mmol, 1.2 equiv., condensed at −78° C.). The solution was sealed and stirred over 20 hours, during which time the temperature warmed to room temperature. The reaction mixture was concentrated in vacuo and the crude product was distilled (75° C., 0.5 torr) to provide 2-(3,3-dimethyl-morpholin-4-yl)-ethanol (14 g, 82%) as a colorless oil contaminated with ˜15% of 3,3-dimethyl-morpholine. LC/MS found 160.10 (M++H, C8H18NO2 requires 160.13).
後処理
- customThe solution was sealed
- concentrationThe reaction mixture was concentrated in vacuo
- distillationthe crude product was distilled (75° C., 0.5 torr)
出典と根拠
- ORDレコード
- ord-91cc488779f54d01b7f4e6c365528db3
- 出典データセット
- uspto-grants-2014_08
- 特許番号
- US08809266B2
反応ノート
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